摘要
建立了一种采用高效液相色谱-电感耦合等离子体串联质谱联用仪测定大米中硒代胱氨酸(SeCys_(2))、甲基-硒代半胱氨酸(MeSeCys)、亚硒酸根[Se(Ⅳ)]、硒代蛋氨酸(SeMet)及硒酸根[Se(Ⅵ)]5种硒形态的分析方法。利用小麦粉质控样(ERM-BC210a)中硒代蛋氨酸的测定回收率分析优化硒形态的提取效果;以O2作为反应池气体,在硒元素质量转移Se(m/z 80>96)模式下,以Hamilton PRP-X100为分析柱,以5 mmol·L^(-1)的柠檬酸溶液(pH=5.0)为流动相,采用高效液相色谱-电感耦合等离子体串联质谱联用法检测。结果表明,在0.5~200.0μg·L^(-1),各硒形态线性关系良好,相关系数均大于0.9995;SeCys_(2)、MeSeCys、Se(Ⅳ)、SeMet和Se(Ⅵ)检出限分别为0.002、0.004、0.005、0.002 mg·kg^(-1)和0.001 mg·kg^(-1);在0.025、0.100、0.250 mg·kg^(-1)3个加标水平下,各硒形态的平均加标回收率为79.9%~106.3%。10批海南地区大米中主要检出的硒形态为SeMet,其他硒形态均未检出。该方法准确、灵敏,可满足大米中硒形态的定量分析。
A method was developed for the determination of five selenium forms in rice,including selenocystine(SeCys_(2)),methyl-selenocysteine(MeSeCys),selenite[Se(Ⅳ)],selenomethionine(SeMet)and selenate[Se(Ⅵ)],by high performance liquid chromatography-inductively coupled plasma tandem mass spectrometry.The recovery rate of selenomethionine in wheat flour quality control sample(ERM-BC210a)was used to analyze and optimize the extraction effect of selenium morphology.O2 was used as the reaction cell gas,selenium mass transfer Se(m/z 80>96)mode,Hamilton PRP-X100 was used as the analytical column,and 5 mmol·L^(-1) citric acid solution(pH=5.0)was used as mobile phase and was detected by high performance liquid chromatography-inductively coupled plasma tandem mass spectrometry.The results showed that in 0.5 to 200.0μg·L^(-1),the linear relationship between selenium morphology was good,and the correlation coefficients were greater than 0.9995,and the detection limits of SeCys_(2),MeSeCys,Se(Ⅳ),SeMet and Se(Ⅵ)were 0.002 mg·kg^(-1),0.004 mg·kg^(-1),0.005 mg·kg^(-1),0.002 mg·kg^(-1) and 0.001 mg·kg^(-1),respectively.The average recoveries of selenium forms were from 79.9%to 106.3%at the three spike levels of 0.025 mg·kg^(-1),0.100 mg·kg^(-1) and 0.250 mg·kg^(-1).SeMet was the main selenium form detected in 10 batches of rice from Hainan,while no other selenium forms were detected.This method is accurate and sensitive,which can meet the quantitative analysis of selenium form in rice.
作者
符郁馥
韦盈
刘冬妮
康蕊
林志藩
谷满屯
FU Yufu;WEI Ying;LIU Dongni;KANG Rui;LIN Zhifan;GU Mantun(Institute of Food Testing,Hainan Academy of Inspection and Testing,Key Laboratory of Tropical Fruits and Vegetables Quality and Safety,State Administration for Market Regulation,Haikou 570314,China)
出处
《食品安全导刊》
2025年第1期87-92,共6页
China Food Safety Magazine
基金
海南省自然科学基金青年基金项目(320QN375)
国家市场监督管理总局重点实验室(热带果蔬质量与安全)课题资助项目(ZZ-2022002)。
关键词
硒形态
大米
高效液相色谱-电感耦合等离子串联质谱联用仪
selenium species
rice
high performance liquid chromatography-inductively coupled plasma tandem mass spectrometry
